Department of Chemistry, Shahid Beheshti University, Tehran, Iran.
J Sep Sci. 2013 May;36(9-10):1597-603. doi: 10.1002/jssc.201201099. Epub 2013 Apr 2.
A rapid and simple quantitative method for preconcentration and determination of haloperidol in biological samples was developed using ultrasound-assisted emulsification microextraction, based on the solidification of floating organic droplet combined with HPLC-DAD. The effects of several factors were investigated. A total of 30 μL of 1-undecanol as an extraction solvent was injected slowly into a glass-centrifuge tube containing 4 mL alkaline sample solution that was located inside the ultrasonic water bath. The formed emulsion was centrifuged and the fine droplets of solvent were floated at the top of the test tube, then it was cooled in an ice bath and the solidified solvent was transferred into a conical vial, after melt, the analysis of the extract was carried out by HPLC. Under the optimal conditions, the extraction efficiencies were more than 90% and the preconcentration factors were obtained between 119-122. The LOQs were obtained between 4-8 μg/L and the calibration curves were linear within the range of 4-1000 μg/L. Finally this method was applied to the determination of haloperidol in plasma and urine samples in the range of μg/L and satisfactory results were achieved (RSDs <7%).
建立了一种基于超声辅助乳化微萃取-顶空固相微萃取结合高效液相色谱-二极管阵列检测法快速、简单测定生物样品中甲哌啶醇的方法。考察了多种因素的影响。将 30μL 十一醇缓慢注入到含有 4 mL 碱性样品溶液的玻璃离心管中,该离心管位于超声水浴中。形成的乳状液在离心作用下,溶剂的细小液滴会浮在试管顶部,然后在冰浴中冷却,使凝固的溶剂转移到锥形小瓶中,在融化后,通过高效液相色谱进行萃取分析。在最佳条件下,萃取效率大于 90%,预浓缩因子在 119-122 之间。LOQs 在 4-8μg/L 之间,校准曲线在 4-1000μg/L 范围内呈线性。最后,该方法应用于血浆和尿液中甲哌啶醇的测定,μg/L 范围内得到了满意的结果(RSDs <7%)。